EP2134884A2 - Procédé d'application d'un revêtement à résistance élevée sur des pièces à usiner et/ou des matériaux - Google Patents

Procédé d'application d'un revêtement à résistance élevée sur des pièces à usiner et/ou des matériaux

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Publication number
EP2134884A2
EP2134884A2 EP08736109A EP08736109A EP2134884A2 EP 2134884 A2 EP2134884 A2 EP 2134884A2 EP 08736109 A EP08736109 A EP 08736109A EP 08736109 A EP08736109 A EP 08736109A EP 2134884 A2 EP2134884 A2 EP 2134884A2
Authority
EP
European Patent Office
Prior art keywords
coating
layer
workpiece
materials
workpieces
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP08736109A
Other languages
German (de)
English (en)
Other versions
EP2134884B1 (fr
Inventor
Oliver Nöll
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SURCOATEC AG
Original Assignee
Stein Ralf
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Filing date
Publication date
Application filed by Stein Ralf filed Critical Stein Ralf
Publication of EP2134884A2 publication Critical patent/EP2134884A2/fr
Application granted granted Critical
Publication of EP2134884B1 publication Critical patent/EP2134884B1/fr
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • C23C16/029—Graded interfaces
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T50/00—Aeronautics or air transport
    • Y02T50/60—Efficient propulsion technologies, e.g. for aircraft
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
    • Y10T428/2848—Three or more layers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31678—Of metal

Definitions

  • the present invention relates to a method for applying a coating to workpieces and / or materials according to the preamble of claim 1.
  • Such coatings are applied to workpieces and / or materials in particular by plasma coating methods such as the "Plasma Enhanced Chemical Vapor Deposition” (PECVD) method.
  • PECVD Plasma Enhanced Chemical Vapor Deposition
  • This process is a special form of "Chemical Vapor Deposition” (CVD), in which the deposition of thin layers by chemical reaction takes place in a vacuum chamber; In this case, the material with which the coating is to be carried out, in the gas or vapor phase before.
  • PECVD is supported by a plasma.
  • a strong electric field is applied between the substrate to be coated and a counter electrode, through which a plasma is ignited.
  • the plasma causes a breakdown of the bonds of the reaction gas and decomposes it into ions or radicals, which precipitate on the substrate and cause the chemical precipitation reaction there.
  • a higher deposition rate can be achieved at a lower deposition temperature than with CVD.
  • This type of coating is therefore particularly suitable for punching, cutting, drilling and screwing tools, cutting tools, prostheses, ball or roller bearings, gears, pinions, drive chains, sound and drive units in magnetic recording devices, as well as surgical and dental surgical instruments.
  • it is suitable for blades with exchangeable blades, e.g. surgical knives, and / or blades and / or knives for industrial applications.
  • the workpieces to be coated and / or materials may in particular consist of metals, ceramics or plastics, have such materials, or else represent mixtures or composites of said materials.
  • the workpieces and / or materials to be coated have a different residual stress than the coating. This is due to the nature of the production. For example, hard metal workpieces or materials suffer from extreme internal stress or, depending on the composition, are subject to very high residual stresses during the flame spraying process.
  • powder mixtures are used, which in the way do not allow a subsequent DLC coating in the true sense, these repel even if they must be carbon-free or should.
  • HSS HSS
  • Object of the present invention is therefore to provide a well-adherent coating for workpieces and / or materials that gives them on the surface a high hardness, high toughness, high resistance to tribological stresses, high smoothness and a low coefficient of friction, and which is also resistant to point loads.
  • Another object of the present invention is to provide a well-adherent coating for workpieces and / or materials which is resistant to point loads and at the same time has suitable surface properties with respect to surface tension and resistance to paints and cleaning agents such as acids and alkalis, electrical insulating and heat-conducting properties , and / or has biocompatibility and antiallergic properties.
  • Another object of the present invention is to provide a well-adherent coating for cutting, chip, drilling, forging, milling, screwing and punching tools, which has a long service life and / or life.
  • Another object of the present invention is to provide a well-adhering life and / or life-prolonging coating which is suitable for blades having a high sharpness.
  • a method for applying a coating to workpieces and / or materials comprising the following steps:
  • the workpiece or material may consist in particular of ceramic, iron, steel, high-alloy steel, nickel, cobalt and their alloys with chromium, molybdenum and aluminum, copper and copper alloys, titanium or alloys comprising the aforementioned materials. Furthermore, the workpiece or the material of metals and / or metallic alloys based on Zn, Sn, Cu, Fe, Ni, Co, Al, Ti, and the refractory metals such as Mo, W, Ta etc . Next come sintered metal materials and Metal-ceramic composites (MMC) and metal-polymer composites as well as ceramic materials of oxides, carbides, borides and nitrides in question.
  • MMC Metal-ceramic composites
  • the workpiece may also consist of plastic or a plastic mixture.
  • plastic or a plastic mixture.
  • alloys or composites of the mentioned materials come into question.
  • the high-strength cover layer is applied by plasma coating.
  • a carbon- or silicon-containing reaction gas such as methane (CH 4 ), ethene (C 2 H 4 ), acetylene (C 2 H 2 ), methyl-trichloro-silane (CH 3 SiCl 3 ) or tetramethyldisiloxane (C 4 H 14 OSi 2 ).
  • a carbonaceous overcoat which often has diamond-like properties and structures and is therefore also referred to as a diamond-like carbon (DLC) layer
  • DLC diamond-like carbon
  • a silicon nitride film as a cap layer is formed by using the reaction gases ammonia and dichlorosilane.
  • the reaction gases silane and oxygen are used.
  • Such layers are also particularly preferred embodiments of the invention.
  • tungsten hexafluoride (WF 6 ) is used as the reaction gas, for example.
  • Titanium nitride layers as a topcoat for hardening tools are made of TDMAT (Tetrakis dimethyl amido titanium) and nitrogen. Silicon carbide layers are deposited from a mixture of hydrogen and methyl trichlorosilane (CH 3 SiCIs).
  • titanium-containing layers wherein as the starting material preferably titanium isopropoxide (Ci 2 H 2S O 4 Ti) is used.
  • the adhesive layer of the invention contributes in various ways to improved adhesion of the cover layer on the workpiece or material. So
  • the intermediate layer is applied with the residual stress verquer to the residual stress of the material, ie the substrate and thus has a balancing effect.
  • the workpiece to be coated or the material to be coated consists of metal, in particular of steel or stainless steel, aluminum or titanium and their alloys.
  • the surface of these metals is relatively soft and easily plastically deformable compared to the applied high strength carbon or silicon containing overcoat.
  • the said cover layer is extremely hard, but it is brittle. In some situations, for example extremely high point loads, this leads to the workpiece or the material being plastically deformed and the cover layer, due to its brittleness, can not follow this deformation, but it breaks or bursts.
  • Tools and materials that are coated with such a top layer so have in certain applications and load scenarios low lifetimes and / or life.
  • support layers do not exhibit the extreme hardness of the cover layer, but have sufficiently tough properties that they do not yield at high point loads, thus preventing breakage or spalling of the cover layer.
  • the properties of said support layer will be discussed below.
  • step b) the step
  • step a.2) can therefore be carried out before and / or after the step a.1).
  • sputtering or “sputter etching” refers to a physical process in which atoms are dissolved out of a solid by bombardment with high-energy ions and pass into the gas phase. These ions are often - similar to the PECVD - by generating a plasma by means of a high-frequency alternating electromagnetic field in a vacuum chamber generated.
  • noble gases are generally suitable as the reaction gas, for example argon (Ar 2 ).
  • Ar 2 argon
  • oxygen (O 2 ) for non-ferrous materials such as brass, bronze, aluminum etc. a mixture of oxygen (O 2 ) and hydrogen (H 2 ).
  • a mixture of H 2 and O 2 is also used if the subsequent intermediate layer or the substrate to be coated requires it.
  • Ion etching allows the substrate surface to be cleaned down to the nanoscale and removed in a nominal sense. This removal of the surface can be measured, for example, with the aid of O 2 after a short time and moves per hour in the range of 100 nm. This ensures that the substrate surface to be treated is free of all impurities.
  • the use for cleaning the surface in the broadest sense even the activation, by a mixture of H 2 and O 2 necessary to achieve any adhesion.
  • said support layer by at least one method selected from the group
  • the heat to melt the powder is by the reaction of oxygen and fuel gas, such as gasified kerosene, in the Combustion chamber generated.
  • the temperatures reached in the flame are up to about 3000 0 C.
  • the reaction expands the gas and accelerates the spray powder to a high speed.
  • a plasma torch In plasma spraying, a plasma torch is usually used in which an anode and cathode are separated by a narrow gap. A DC voltage creates an arc between the anode and the cathode. The gas flowing through the plasma torch is passed through the arc and thereby ionized. The ionization, or subsequent dissociation, generates a highly heated (up to 20,000 K), electrically conductive gas of positive ions and electrons. In this Plasmajet produced powder is injected, which is melted by the high plasma temperature. The plasma gas stream entrains the powder particles and hurls them at a speed of up to 1000 m / s onto the workpiece to be coated.
  • the gas molecules return to a stable state after only a short time, no longer release any energy, and so the plasma temperature drops again after a short distance.
  • the plasma coating is usually carried out under atmospheric pressure.
  • Gases used are argon, helium, hydrogen, oxygen or nitrogen.
  • Flame spraying with powder is the oldest method of thermal spraying technology. Due to the fuel gas / oxygen flame as a heat source only low melting metals and alloys can be processed. By flame spraying with subsequent melting of e.g. Nickel- or cobalt-based hard alloys can achieve dense and thick layers up to 2.5 mm. Additions of carbides cause a significant increase in hardness.
  • the coating material is present as a powder.
  • metal-bound carbides such as tungsten carbide, chromium carbide, titanium carbide, silicon carbide, or oxides, such as aluminum oxide, titanium dioxide, chromium oxide, magnesium oxide, zirconium oxide and their alloys and mixtures.
  • the coating material is present as a wire.
  • the coating material is applied by the fuel gas / oxygen flame and the gas velocity.
  • Typical coating materials in this process are metals, eg molybdenum, Cr steel, Cr-Ni steel, Zn, etc.
  • Anodizing is a process whereby an oxide protective layer is applied to an aluminum workpiece or material, which is applied by anodic oxidation, whereby the protective layer is not deposited on the workpiece, in contrast to the galvanic coating method but by converting the uppermost metal zone into an oxide or hydroxide, a 5 to 25 micron thin layer is formed to protect the aluminum from corrosion, while the natural oxide layer of aluminum is only a few nanometers thick about 8-9 according to the hardness scale of Mohs, ie between quartz and corundum.
  • Oxidation of aluminum surfaces which is produced in strongly cooled electrolytes. This coating is characterized by high wear, heat, corrosion and electrical resistance. In addition, there are good sliding properties with greatly reduced mass forces. Since the hard-enamel layer is formed from the base material itself, there are no adhesion problems. The good wear properties are due to the forming during the process of alumina from the Harteloxal- layer. Hard anodising is used for extruded profiles and turned parts as well as for pressure, sand and chill casting, forging and wrought alloys. This term encompasses several anodization techniques that can be used to produce thick (50-100 ⁇ m) and dense oxide layers at low temperature.
  • Electroplating is understood to mean the electrochemical deposition of metallic precipitates on workpieces or materials. In this case, electricity is sent through an electrolytic bath.
  • the metal to be applied eg copper, nickel, cobalt, manganese, chromium or certain alloys
  • the electric current dissolves metal ions from the consumable electrode and stores them by reduction on the goods.
  • the object to be refined is uniformly coated on all sides with copper or another metal. The longer the object is in the bath and the higher the electrical current, the stronger the metal layer becomes (eg copper layer).
  • the surface hardness of the workpiece or material can be increased in this way.
  • Powder coating is a coating process in which a usually electrically conductive material or a workpiece is coated with powder coatings.
  • the powder is sprayed electrostatically or tribostatically on the substrate to be coated and then baked.
  • the workpiece is to be degreased well and, if necessary, treated with corrosion protection.
  • the baking temperatures depending on the application, vary widely. Typical baking conditions are between 140 and 200 ° C.
  • Various binders are used today, but typical are powder coatings based on, for example, polyurethane, epoxy or polyester resins. Because of the
  • the powder can also be applied by vortex sintering. In this case, a heated workpiece is immersed briefly in a fluidized by means of compressed air powder made of plastic. The powder melts on the surface to a
  • various of the mentioned methods can also be combined.
  • a combination of electrophoretic and electrodeposition in successive steps. For example, first, a ceramic layer (for example, yttrium-stabilized zirconia) electrophoretically produced on a workpiece and then sintered at 1100 0 C for an open-porous layer. The next step is then through Galvansieren example, nickel deposited in the pores of the layer. By a final thermal treatment, the connection of the composite support layer thus produced to the workpiece or the material is improved.
  • a ceramic layer for example, yttrium-stabilized zirconia
  • the basic principle of electrophoresis is the migration of dispersed particles in a DC electric field and their deposition on an electrode.
  • ceramic powders such as yttrium oxide Y 2 O 3 and titanium oxide
  • the coating is usually carried out at a DC voltage of 5 - 200 V.
  • a coating substrate to be coated workpiece or the material which also acts as an electrode.
  • the counter electrode consists e.g. made of graphite.
  • said support layer is at least one layer selected from the group
  • chromium (VI) layer • chromium (VI) layer, and / or
  • An anodized layer is a layer applied by the anodizing method already mentioned. Ceramic layers can be treated with various of the mentioned methods be applied, in particular with the said spraying method and the electrophoretic method.
  • a chromium (V ⁇ ) layer is usually applied by electroplating.
  • Corundum layers consist of Al 2 O 3 and are considered to be the second hardest mineral with a Mohs hardness of 9 after the diamond. Corundum is considered as technical ceramics and is also applied as a coating on a workpiece or a material, for example, with the said spraying method and the electrophoretic method.
  • the adhesive layer is applied by means of plasma coating on the workpiece and / or the material.
  • Said adhesive layer preferably has elements from the 6th and / or 7th subgroup. Preference is given here to compounds which contain the elements Cr, Mo, W, Mn, Mg, Ti and / or Si, and in particular mixtures thereof. Likewise, the individual constituents can be distributed in graded form over the depth of the adhesive layer. Particularly preferred here is Si. As reaction gas here comes e.g. the highly volatile TMS under vacuum conditions.
  • Step a.2) in this embodiment represents a multi-gas sputtering process, the advantages of which will be discussed later.
  • step b) and / or step c) is carried out under an inert and / or a reducing atmosphere.
  • the deposition in steps b) and / or c) can take place under a protective gas atmosphere, for example by simultaneous feeding of Ar 2 .
  • the chamber is purged with a protective gas such as Ar 2 in order to displace any remaining residues of an oxidizing gas such as O 2 from the chamber and / or to initiate a rinse with nitrogen as a transfer
  • step b) During the transition from step b) to step c)
  • counter-rotating ramps in the context of the present invention is intended to mean that during the sputtering or PEC VD process, the minute volume of at least one reaction gas is stepped or continuously reduced while the minute volume of another gas is stepped or continuously increased becomes.
  • step a.2) sputtering
  • step c) PECVD
  • the ramps have the effect that the deposition phases of two materials merge. In this way transition areas are created with gradually changing proportions of the various coating materials. This leads to a closer interlocking of the two layers with each other and thus e.g. to a better adhesion of the cover layer to the adhesive layer.
  • the central nature of said ramps is that coordinated in time a gradual transition from at least one reaction gas to at least one other reaction gas coating medium for the intermediate layer to the coating gas for the cover layer must be adjusted fluently with a certain temporal gradient. The same may apply to the change in the bias number and possibly for further coating parameters. So it must be ensured that before each transition of the reaction gases, the chamber is raised or lowered to the desired bias value, in turn, to reduce the formation of residual stress.
  • the abrupt setting of the bias value must be at least 5 seconds before the start of the setting of the gradient, but at the latest 15 seconds before the same.
  • step b) to step c) can be designed, for example, so that first a silicon-containing adhesive layer is applied by plasma coating.
  • a silicon-containing adhesive layer is applied by plasma coating.
  • the liquid at room temperature, but under hypobaric conditions highly volatile tetramethyldisiloxane (C 4 Hi 4 OSi 2 ) is used. After a while, that will be Gas minute volume for TMS successively reduced and the gas minute volume for the Kolhenstoff ambience gas acetylene (ethene) successively increased.
  • Said ramp could look like this: After an optional sputtering step (a.2), the bias voltage V ⁇ ias is raised to the height required for the coating 5 seconds before the start of the application of the intermediate layer. Thereafter, the silane-containing, vaporized gas TMS is introduced with an extremely short ramp (10 s). After the adhesive layer deposition time has elapsed, the acetylene valve is gradually opened to the desired inlet value over a period of 500 seconds. At the same time, the valve for TMS gradually closes in the same time. Subsequently, the cover layer is applied over the desired time. Table 1 gives this method with exemplary values:
  • the application of the cover layer can in principle take any length.
  • the thickness of the cover layer grows proportionally with the duration of the coating. For this reason, the variable "X" was selected as the time value in the above table.
  • ramps are driven in relation to the materials used for the adhesive layer.
  • one material is successively replaced by another.
  • the gas concentration in the chamber results in each case from the gas flow, the volume of the chamber and the pressure prevailing therein.
  • a concentration of 0.011 results for acetylene (C 2 H 2 ) at a gas flow of 100 sccm (0.1175 g per minute) % of the chamber volume.
  • a DLC layer thus prepared using acetylene as a reaction gas has a hardness of 6000-8000 HV and a thickness of 0.90 ⁇ m to 5.0 ⁇ m.
  • O 2 is an attractive reaction gas for sputtering because the ionized oxygen atoms have high kinetic energy due to their high molecular weight and therefore could effectively purify a surface. In addition, oxygen is very cheap.
  • O 2 comes at best for the sputtering of plastic surfaces in question, since a passivation of the surface by oxidation is not to be feared.
  • a further reason for the non-use of O 2 during sputtering is for the expert when, subsequent to the sputtering, a carbon-containing layer is to be applied to the workpiece and / or the material by plasma coating. Any residual O 2 would oxidize carbon to CO and / or CO 2 , resulting in the formation of voids, gas bubbles and microcavities in the carbonaceous layer, creating a rough, less dense and less resilient surface and significantly affecting the adhesion of the topcoat ,
  • Ar 2 also has disadvantages, since it results in a very rough surface during sputtering, which makes it difficult to apply a cover layer such as a DLC layer.
  • the reaction gas contains in step a.2) at least temporarily the gases H 2 and O 2 .
  • the H 2 contained in the reaction gas ensures that the oxidizing effect of O 2 is reduced and a passivation of the metal surfaces does not occur.
  • the molecular weight of the O 2 is ideal to provide an effective cleaning effect during sputtering without, however, roughening the surface of the workpiece and / or material.
  • the electromagnetic alternating field can be shut down during this time. Alternatively, it may be attempted to keep the duration of this washing step as short as possible.
  • the application of the cover layer can in principle take any length.
  • the thickness of the cover layer grows proportionally with the duration of the coating. For this reason, the variable "X" was selected as the time value in the above table.
  • a step (a.l) may be connected for the application of a support layer.
  • This step may e.g. which involves the application of a method selected from the group
  • the method is carried out in a plasma coating chamber, comprising a flat high-frequency electrode for generating an alternating electromagnetic field, and a frequency generator arranged outside the chamber, characterized in that the high-frequency electrode has at least two supply lines, via which it is supplied with an alternating voltage generated by the frequency generator.
  • Such a plasma coating chamber is described for the first time in the applicant's PCT / EP2007 / 057117 of the present invention.
  • an alternating field with very high field strengths can be generated in the chamber.
  • An alternating field generated in this way has a sufficiently high penetration depth and a high degree of homogeneity.
  • homogeneous plasma in all areas of the chamber homogeneous plasma and thus achieves a homogeneous deposition rate, which manifests itself in a constant layer thickness and, as a result, in low residual stress differences within the coating thus produced. Both factors further improve the adhesion of the high-strength cover layer to be applied according to the invention.
  • three or more leads are provided, as can be set in this way an even more homogeneous alternating field.
  • the individual supply lines to the high-frequency electrode be adjusted separately, such that in the entire chamber, a homogeneous
  • the same bias voltage is set on all controllers, which suggests identical field strengths and thus a homogeneous alternating field.
  • a plasma coating chamber comprising a flat high-frequency electrode for generating an alternating electromagnetic field, a frequency generator arranged outside the chamber, and at least two leads, via which the high-frequency electrode is supplied with an alternating voltage generated by the frequency generator, for applying a coating on workpieces and / or materials according to one of the preceding method claims.
  • the subject of the present invention is moreover a coating on workpieces and / or materials, comprising the following layers:
  • adhesive and cover layer have a graduated transition region, or a coating on workpieces and / or materials, produced by a method according to the invention.
  • said coating also has a support layer which is arranged between the workpiece and / or material and the adhesive layer.
  • a support layer which is arranged between the workpiece and / or material and the adhesive layer.
  • the subject of the present invention is an instrument, workpiece or material or component which is coated with one of the aforementioned methods or with an aforementioned coating.
  • This instrument may be e.g. to act a surgical instrument, such as a surgical instrument. a scalpel. Likewise, this instrument can be a punching tool. Furthermore, the instrument may be e.g. to trade a butcher or slicer cutting tool
  • cutting tools coated according to the invention retain their sharpness considerably longer, even if they are used under adverse circumstances. This is especially true for butchery or slaughtering cutting tools, on the one hand soft material (fat, muscle, skin, connective tissue) must cut, on the other hand, however, also hard material such as bone and frozen.
  • soft material fat, muscle, skin, connective tissue
  • hard material such as bone and frozen.
  • surgical instruments which must be sterilized frequently, which leads to severe corrosion in instruments not coated according to the invention after a short time due to the sterilization conditions (heat, humidity and pressure).
  • the suitability of the instrument is impaired as such, and on the other hand suffers in particular the sharpness of the blades used heavily.
  • Cylinder the sealing elements and the surfaces of rods and cylinders.
  • Engine units and components in particular pistons with or without piston rings, liners and cylinder liners, valves and camshafts, pistons and connecting rods.
  • Prostheses implants, screws, plates, artificial joints, stents, biomechanical and micromechanical components.
  • Operative cutlery which generally have to be anti-allergenic, such as scalpels, forceps, endoscopes, cutting instruments, staples etc.
  • Components which must have chemically resistant surfaces against printable inks and cleaning agents and whose surfaces require defined non-stick and liquid-repellent and / or liquid-adhering properties for defined ink dosing, such as rollers, cylinders and scrapers of printing presses.
  • Moving media guides for gas, liquids and gas or liquid fluidized solid media • Moving media guides for gas, liquids and gas or liquid fluidized solid media.
  • workpieces and / or materials to be coated according to the invention include cutting, drilling and screwing tools, cutting tools, ball or roller bearings, gears, pinions, drive chains, sound and drive units in magnetic recording devices, as well as surgical and dental surgical instruments
  • Standard cubic centimeters per minute and represents a standardized volume flow. In vacuum pump technology, one also speaks of the gas load. Regardless of pressure and Temperature is detected with this standard a defined flowing gas quantity (particle number) per unit time.
  • a butcher blade coated with the described method had a threefold service life in comparison to a conventional coater knife with combination coating.
  • An industrial cutting knife for potatoes coated with the described method exhibited an eight times longer service life than a conventional cutting knife with a combination coating.
  • a punching tool coated with the described method for the production of electrical connectors for the automotive industry had a two-fold extended service life compared to a conventional punching tool.
  • Fig. 1 shows a timing chart of the course of the ramps described in Table 4.
  • the first block shows the sputtering step (a.2), while the second block shows the step b) for the application the adhesive layer and the ramp-like toothing of the same with the applied in step c) cover layer.
  • step (a.2) - or even instead of the sputtering step (a.2) - step (a.1) can be connected for the application of a support layer.
  • This step may e.g. the application of a method selected from the group
  • FIGS. 2 to 4 show the results of the physical analysis of three stainless steel workpieces, one of which is provided with a titanium nitride coating ("TiN”) and two further coatings according to the invention ("M44", layer thickness 0.81 ⁇ m, "M59”). , Layer thickness 0.84 ⁇ m, layer structure: DLC cover layer with adhesive layer on a HVOF coating of metal-bonded tungsten carbide type WC-Co 83 17). Titanium nitride is considered in the art as one of the hardest and most resistant coatings for cutting, milling and punching tools.
  • Counter body WC co-ball, diameter 6 mm
  • Friction track diameter D 2 mm
  • Fig. 2 shows the results of the determination of the friction coefficient ⁇ . It can be clearly seen that the coating according to the invention with an average coefficient of friction ⁇ of approximately 0.3 has significant advantages over the TiN coating, whose mean coefficient of friction is almost twice as high throughout.
  • FIG. 3 shows the light microscopic documentation (magnification: 100 ⁇ ) of the wear in the rubbing track after 30,000 revolutions in the case of the coating M59 according to the invention (FIG. 3 a) and of the TiN coating (FIG. 3 b). It is clearly evident here that the coating according to the invention shows significantly lower wear than the TiN coating.
  • FIG. 5 shows an electron micrograph of a section of a workpiece coated according to the invention at a magnification of 3000 times.
  • the DLC layer 1 the bright line emerging adhesive layer 2 and the support layer 3 (here a HVOF support layer).
  • the DLC layer has a thickness of about 4 ⁇ m. It is also clear that the embedding medium adheres poorly to the DLC layer; Thus, the DLC layer has separated during the cutting of the embedding medium (gap 4). It can also be seen that the DLC coating applied by the plasma coating method is able to compensate for unevennesses (5) of the previously applied supporting layer.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)
  • Coating By Spraying Or Casting (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention concerne un procédé d'application d'un revêtement sur des pièces à usiner et/ou des matériaux, présentant les étapes suivantes d'application d'une couche adhésive; ainsi que l'application d'une couche de finition à résistance élevée grâce à un revêtement par plasma.
EP20080736109 2007-04-13 2008-04-11 Procédé d'application d'un revêtement à résistance élevée sur des pièces à usiner et/ou des matériaux Active EP2134884B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102007017891 2007-04-13
DE200710047629 DE102007047629A1 (de) 2007-04-13 2007-10-04 Verfahren zum Aufbringen einer hochfesten Beschichtung auf Werkstücke und/oder Werkstoffe
PCT/EP2008/054394 WO2008125607A2 (fr) 2007-04-13 2008-04-11 Procédé d'application d'un revêtement à résistance élevée sur des pièces à usiner et/ou des matériaux

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EP2134884A2 true EP2134884A2 (fr) 2009-12-23
EP2134884B1 EP2134884B1 (fr) 2012-08-01

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US (2) US20090011252A1 (fr)
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JP (1) JP2010523824A (fr)
KR (1) KR20100016486A (fr)
CN (1) CN101711288A (fr)
AU (1) AU2008237924A1 (fr)
CA (2) CA2629117A1 (fr)
DE (2) DE102007047629A1 (fr)
RU (1) RU2009137553A (fr)
WO (2) WO2008125606A1 (fr)
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JP2010523824A (ja) 2010-07-15
CA2629117A1 (fr) 2008-10-13
WO2008125606A1 (fr) 2008-10-23
CN101711288A (zh) 2010-05-19
US20090011252A1 (en) 2009-01-08
RU2009137553A (ru) 2011-04-20
WO2008125607A2 (fr) 2008-10-23
CA2684019A1 (fr) 2008-10-23
DE102007058484A1 (de) 2008-10-16
AU2008237924A1 (en) 2008-10-23
WO2008125607A3 (fr) 2009-05-07
ZA200907082B (en) 2010-07-28
DE102007047629A1 (de) 2008-10-16
EP2134884B1 (fr) 2012-08-01
KR20100016486A (ko) 2010-02-12
US20100297440A1 (en) 2010-11-25

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